Preparation method of zirconium boride ceramic fibre

Abstract

The invention relates to a preparation method of zirconium boride ceramic fibre, comprising the following steps of: (1) adding an aqueous solution containing a zirconium compound to an aqueous solution containing a boron compound, mixing evenly, dissolving a carbon source compound in the mixed solvent of ethanol and water, adding the mixed solvent of ethanol and water to the solution, adding an aqueous solution of complexing agents, mixing evenly, regulating pH value to be less than 4, and stirring for reaction for 10-16 hours to obtain a precursor solution; (2) mixing evenly a spinning addition agent and the precursor solution at the temperature between 30 and 70 DEG C and concentrating and defoaming the obtained mixture to obtain a precursor spinning solution of the zirconium boride ceramic fibre; (3) obtaining a precursor of the zirconium boride ceramic fibre from the spinning solution by a solvent spinning method at the temperature between 30 and 70 DEG C; and (4) obtaining the zirconium boride ceramic fibre by performing high temperature sintering on the precursor fibre. By adopting the method, ZrB2 ceramic nascent fiber with a better structure and performance can be obtained and the fiber with a promising prospect has the advantages of high temperature stability, low density, high heat conductivity and conductivity and the like.

Description

technical field [0001] The invention belongs to the field of preparation of zirconium boride ceramics, in particular to a preparation method of zirconium boride ceramic fibers. Background technique [0002] Modern aircraft (such as spacecraft, rockets, missiles, supersonic aircraft) are developing towards high speed, high altitude, high thrust and safer, which puts forward higher requirements for high-temperature materials: being able to adapt to supersonic long-term flight, Extreme environments such as atmospheric reentry, transatmospheric flight, and rocket propulsion systems must not only be able to withstand high temperatures (>2000°C), but also require anti-oxidation, anti-scouring, and thermal shock resistance, especially for aircraft nose cones, wing leading edges, Various critical parts or parts such as the hot end of the engine need to use ultra-high temperature materials. [0003] ZrB 2 As a member of ultra-high temperature ceramic materials (UHTCs), it has hi...

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Problems solved by technology

[0005] ZrB 2 Although it has many superior characteristics, its current performance cannot meet the needs of practical applications. 2 The research mainly focuses on the preparation of raw material powder, the sintering densification process and the preparation of composite materials to improve its mechanical properties and high temperature oxidation resistance.

However, at present, there are few studies on ZrB at home and abroad. 2 Related reports on the preparation of ceramic fibers and their composite materials, Yuriy B.Paderno et al. (Y.B.Paderno et al.Journal of the European Ceramic Society, 2005, 25, 1301-1305.) used diboride eutectic directional solidification to prepare a single Crystal form of submicron ZrB 2 、TiB 2 and HfB 2 fiber, ZrB 2 The fiber diameter is 0.4-0.8 microns, the aspect ratio is up to 500, and the fiber is uniform and smooth as a whole. The diborides of these fibrous structures have special applications in structural components, functional devices, etc., and may also be used in industrial filter paper and heating protection systems. , reinforcement materials, etc.

[0006] However, there is no direct preparation of ZrB at home and abroad. 2 Report on ceramic fiber method

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